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4-Nitrobenzenesulfonyl chloride → (s)-(4-Nitro-benzenesulfonylamino)-phenyl-acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Nitrobenzenesulfonyl chloride | HCID 7404 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | L-Phenylglycine | HCID 99291 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (s)-(4-Nitro-benzenesulfonylamino)-phenyl-acetic acid | HCID 362697 | — |
反応手順
To a solution of L-phenylglycine (0.227 g, 1.5 mmol) in water (5 ml) and dioxane (5 ml) was added triethylamine (0.42 ml, 3.0 mmol) followed by slow addition of 4-nitrobenzene sulphonyl chloride (0.5 g, 2.3 mmol) in dioxane (5 ml) at 0° C. After stirring for 45 minutes the reaction mixture was evaporated to dryness, re-dissolved in EtOAc and washed with saturated NaHCO3 solution (2×20 ml) and water (10 ml). The EtOAc layer was dried over Na2SO4, filtered and evaporated to dryness. LCMS purity 75%, (molecular ion not observed) yield 0.58 g, (76%). This material was used without any purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07939666B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-e6c50959d0094ca88cc7a704e2bf1aef |
| 出典メモ | uspto-grants-2011_05 |